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Extracting method for abamectin B1a

A technology of abamectin and extraction method, which is applied in the direction of chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problem of affecting the quality and yield of abamectin products, the poor selectivity of macroporous resins, the impact on Abamectin leaching rate and other issues, to achieve the effect of reducing solvent loss, reducing the intensity of environmental protection treatment, and reducing the number of leaching times

Active Publication Date: 2017-05-10
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] (1) When the abamectin mycelium is flash-dried, if the drying temperature is too high, the protein and lipids on the surface of the mycelium will be denatured, thereby changing the permeability of the cells, thereby affecting the abamectin Leaching rate
[0011] (2) Extraction with a single ethanol requires repeated extractions, resulting in large consumption of ethanol and high production costs
[0012] (3) The selectivity of the macroporous resin is not strong, and it has little effect on the separation of each component in the purification process of abamectin Bl
[0013] (4) Petroleum ether / isopropanol is used for solvent recovery, which is difficult to separate and has a large loss of solvent
[0014] (5) In order to improve the purity of abamectin, it is necessary to purify and crystallize many times, and the heating temperature during crystallization is high and the time is long, which affects the quality and yield of abamectin products
[0015] (6) Solvents such as petroleum ether, toluene, and n-hexane are flammable and explosive solvents, and the use of such solvents for leaching poses a greater safety risk

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Take 100L of abamectin fermentation broth (potency 1360 u / ml, total 1.36×10 8 u), enter the microporous membrane, add 1.5 times the amount of dialysis water, and 5 times the concentration, and collect 50L of concentrated solution (titer 2660 u / ml, total 1.33×10 8 u), the yield is 97.79%.

[0044] Transfer the above concentrated solution to the extraction tank, control the temperature at 20°C, add 250L of composite solvent (solvent kerosene: ethanol = 2.2:5.5), extract for 4 hours, collect the extraction solution, and press out the tail solution with nitrogen, and summarize Extraction solution, concentrated by thin film evaporation under reduced pressure to oily liquid, volume 2.2L (potency 59500 u / ml, total 1.31×10 8 u), the yield is 98.49%.

[0045] Add the above oily concentrated solution to the prepared alumina chromatography column, pressurize it with nitrogen gas at 0.05MPa, use butanol as the mobile phase, and analyze the concentrated solution of abamectin at a ...

Embodiment 2

[0049] Take 100L of abamectin fermentation broth (potency 1360 u / ml, total 1.36×10 8 u), enter the microporous filter membrane, add 2.0 times of dialysis water, and 5.5 times of concentration, collect 54.5L of concentrated solution (titer 2440 u / ml, total 1.33×10 8 u), the yield is 97.82%.

[0050] Transfer the above concentrated solution to the extraction tank, control the temperature at 22°C, add 300L of composite solvent (solvent kerosene: ethanol = 2.4:6.0), extract for 4.5 hours, collect the extraction solution, and press out the tail solution with nitrogen. Summarize the extracts, evaporate and concentrate to an oily liquid with a volume of 2.6L (potency 50200 u / ml, total 1.30×10 8 u), the yield is 97.74%.

[0051] Add the above oily concentrated solution to the prepared alumina chromatography column, pressurize it with nitrogen gas at 0.06MPa, use butanol as the mobile phase, and analyze the concentrated solution of abamectin at a flow rate of 0.40BV / h, and collect ab...

Embodiment 3

[0055] Take 100L of abamectin fermentation broth (potency 1360 u / ml, total 1.36×10 8 u), enter the microporous membrane, add 2.5 times the amount of dialysis water, and 6 times the concentration, and collect 58L of concentrated solution (titer 2290 u / ml, total 1.33×10 8 u), the yield is 98.10%.

[0056] Transfer the above concentrated solution to the extraction tank, control the temperature at 23°C, add 100L of composite solvent (solvent kerosene: ethanol = 2.6:6.5), extract for 5 hours, collect the extraction solution, press out the tail solution with nitrogen, and summarize Extraction solution, concentrated by thin film evaporation under reduced pressure to oily liquid, volume 2.9L (potency 45210 u / ml, total 1.31×10 8 u), the yield is 98.49%.

[0057] Add the above oily concentrate to the prepared alumina chromatography column, pressurize it with nitrogen to 0.07MPa, use butanol as the mobile phase, and analyze the concentrate of avermectin at a flow rate of 0.50BV / h, and ...

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Abstract

The invention relates to an extracting method for abamectin B1a. The extracting method is characterized by comprising the following process steps: first, filtering abamectin fermenting liquid by adopting a micro-filtration membrane to obtain abamectin-rich membrane paste; then, extracting the membrane past by using a compound solvent; next, adsorbing by using an aluminium oxide chromatographic column and desorbing by butyl alcohol after the obtained extracting liquid is concentrated; collecting desorbing liquid of a B1 stage, de-colouring, filtering and performing primary crystallizing to obtain abamectin B1 crude product; re-crystallizing through ethyl acetate to obtain a finished product with high content of the abamectin B1a. According to the extracting method, the abamectin is extracted in the mode of adopting micro-filtration membrane and compound solvent extracting and combining an aluminium oxide chromatographic column and butyl alcohol desorbing process, so that the abamectin and the product quality can be effectively improved; moreover, the process is simple; the solvent loss is little; the solvent is easy to recycle; the safety is high; meanwhile, environmental pollution can be reduced.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction, in particular to an extraction method of abamectin B1a. Background technique [0002] Abamectin is a class of 16-membered macrolide compound with insecticidal, acaricidal and nematicidal activities first developed by Satoshi Omura of Kitasato University in Japan and Merck Company of the United States. It is fermented by Streptomyces avermitilis in Streptomyces griseus produce. Abamectin has the characteristics of agriculture, animal husbandry and medicine, and has strong insect repellent and insecticidal activities. It is currently the most effective parasiticide, acaricide and insecticide in the world. Abamectin is easy to degrade under natural conditions, safe for humans and animals, has little effect on natural enemies, and belongs to green biological pesticides. Abamectin is also an ester-soluble antibiotic, which mainly exists in the cells of the bacteria, and only a small am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 裴立忠王勇平宋鲁宁郭佳赵亚宁汤根生
Owner NINGXIA TAIYICIN BIOTECH CO LTD
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